CN101260008A - Method for preparing ureaformaldehyde - Google Patents
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- CN101260008A CN101260008A CNA2007100718657A CN200710071865A CN101260008A CN 101260008 A CN101260008 A CN 101260008A CN A2007100718657 A CNA2007100718657 A CN A2007100718657A CN 200710071865 A CN200710071865 A CN 200710071865A CN 101260008 A CN101260008 A CN 101260008A
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Abstract
A preparation method of urea formaldehyde relates to the improvement of a preparation method of urea formaldehyde, and aims to the change the status quo that most urea formaldehyde preparation processes adopt highly volatile hydrochloric acid as catalyst. The invention comprises the following steps: filtrate is added in a reaction kettle and is heated to 60 DEG C; urea is added and is dissolved through stirring, and then the pH value of the solution is adjusted to 8.5 to 8.8 by means of 20 percent of NaOH solution; formaldehyde is added in with the proportion between formaldehyde and urea ranging between 1:1.2 and 1:1.5, and temperature is heated to 75 DEG C to 78 DEG C; the pH value of the solution is adjusted to 8.5 to 8.8 by means of 20 percent of NaOH solution, and the temperature is kept 60 minutes to 70 minutes and then is dropped to 60 DEG C; then, 20 percent of dilute sulfuric acid is added in to adjust the pH value between 5.4 and 5.1 with the temperature kept at 65 DEG C to 68 DEG C for 10 minutes to 15 minutes; 20 percent of dilute sulfuric acid is added in to adjust the pH value between 4.8 and 4.6 with the temperature kept at 65 DEG C to 68 DEG C for 10 minutes to 15 minutes; 20 percent of dilute sulfuric acid is added in to adjust the pH value between 4.4 and 4.1 with the temperature kept at 65 DEG C to 68 DEG C for 10 minutes to 15 minutes; and finally, 20 percent of NaOH solution is added in to adjust the pH value between 8.0 and 8.5 with the temperature dropped to 30 DEG C, thereby the reaction is finished. The preparation method is used to make urea formaldehyde.
Description
Technical field:
The present invention relates to a kind of preparation method's of urea formaldehyde improvement.
Background technology:
Existing urea formaldehyde preparation technology is catalyzer mostly with hydrochloric acid, but hydrochloric acid volatilization easily itself is wayward, and price is more expensive.Most of dissolved nitrogen in the urea formaldehyde fertilizer that conventional art is produced can run off from soil by leaching, runoff or volatilization and denitrogenation, environment is produced destroy.In addition, the prepared urea formaldehyde product of existing manufacturing technique is based on Powdered, in transportation with use all inconvenient.
Summary of the invention:
The invention provides a kind of is the production method of the urea formaldehyde of catalyzer with sulfuric acid, and the urine formaldehyde that utilizes this method to produce has very strong adjusting controlled-release function, reduces the influence to fertilizer of leaching, runoff, helps the protection of ecotope.
Above-mentioned purpose realizes by following technical scheme:
In reactor, add filtrate, be warming up to 60 ℃, add urea, use 20%NaOH adjust pH to 8.5～8.8 after the stirring and dissolving, add formaldehyde, described formaldehyde, urea ratio are 1: 1.2～1.5, and this moment, temperature rose to 75～78 ℃, with 20%NaOH adjust pH to 8.5～8.8, constant temperature kept 60～70 minutes, open cycle cold water is cooled to 60 ℃ then, adds then between 20% the dilute sulphuric acid adjust pH 5.4～5.1, and constant temperature kept 10～15 minutes for 65～68 ℃; Between the dilute sulphuric acid adjust pH 4.8～4.6 of adding 20%, constant temperature kept 10～15 minutes for 65～68 ℃; Add between 20% the dilute sulphuric acid adjust pH 4.4～4.1, constant temperature kept 10～15 minutes for 65～68 ℃, with 20%NaOH adjust pH to 8.0～8.5, cooled the temperature to 30 ℃, and termination reaction is carried out blowing, centrifugal, oven dry, pulverizing, extruder grain, packing.
This technical scheme has following beneficial effect
1. the slow release fertilizer urea formaldehyde that utilizes the present invention and produced owing to adopt particulate state in appearance, has improved the utilization ratio of nitrogenous fertilizer efficient and plant, reduces the demand of fertilizer then, also helps the protection of ecotope in the time of the expensive day by day energy of protection.
2. the slow release fertilizer urea formaldehyde that utilizes the present invention and produced owing to adopt particulate state in appearance, has been avoided unemployed dissolved nitrogen to run off from soil as far as possible, and then has been protected environment.
3. the slow release fertilizer urea formaldehyde that utilizes the present invention and produced, because the slow releasing function of granulated fertilizer, single-dose application and the season of growth effect of repeatedly topdressing is identical, even better, thereby has saved the labor force, the problem of solution labor shortage.
4. to adopt sulfuric acid be that catalyzer replaces hydrochloric acid in the past in the present invention, because sulfuric acid is diprotic acid, hydrochloric acid is monoprotic acid, and under the condition of same concentrations, the vitriolic consumption is half of hydrochloric acid.
5. to adopt sulfuric acid be that catalyzer replaces hydrochloric acid in the past in the present invention because the hydrochloric acid of same concentrations and sulfuric acid, the vitriolic price be hydrochloric acid half in addition lower, so adopt sulfuric acid can reduce production costs greatly, improve economic benefit of enterprises as catalyzer.
6. to adopt sulfuric acid be that catalyzer replaces hydrochloric acid in the past in the present invention, and under same dilute solution condition, hydrochloric acid has volatility, storing, inconvenience all arranged in the transportation, use, and sulfuric acid can overcome these shortcomings.
Description of drawings:
Accompanying drawing 1 is the schema of technology of the present invention.
The specific embodiment of the present invention:
Embodiment 1:
The preparation method of urea formaldehyde, its technical process is: add filtrate in reactor, be warming up to 60 ℃, add specified amount urea.Use 20%NaOH adjust pH to 8.5 after the stirring and dissolving.Add the formaldehyde of specified amount, described formaldehyde, urea ratio are 1: 1.2～1.5, and this moment, temperature rose to 75 ℃, and with 20%NaOH adjust pH to 8.5, constant temperature kept 60 minutes.Open cycle cold water is cooled to 60 ℃ then, adds then between 20% the dilute sulphuric acid adjust pH 5.4, and constant temperature kept 10 minutes for 65 ℃; Between the dilute sulphuric acid adjust pH 4.8 of adding 20%, constant temperature kept 10 minutes for 65 ℃; Between the dilute sulphuric acid adjust pH 4.4 of adding 20%, constant temperature kept 10 minutes for 65 ℃.With 20%NaOH adjust pH to 8.0, cool the temperature to 30 ℃, termination reaction is carried out blowing, centrifugal, oven dry, pulverizing, extruder grain, packing.
Embodiment 2:
The preparation method of urea formaldehyde, its technical process is: add filtrate in reactor, be warming up to 60 ℃, add specified amount urea.Use 20%NaOH adjust pH to 8.8 after the stirring and dissolving.Add the formaldehyde of specified amount, described formaldehyde, urea ratio are 1: 1.2～1.5, and this moment, temperature rose to 78 ℃, and with 20%NaOH adjust pH to 8.8, constant temperature kept 70 minutes.Open cycle cold water is cooled to 60 ℃ then, adds then between 20% the dilute sulphuric acid adjust pH 5.1, and constant temperature kept 15 minutes for 68 ℃; Between the dilute sulphuric acid adjust pH 4.6 of adding 20%, constant temperature kept 15 minutes for 68 ℃; Between the dilute sulphuric acid adjust pH 4.1 of adding 20%, constant temperature kept 15 minutes for 68 ℃.With 20%NaOH adjust pH to 8.5, cool the temperature to 30 ℃, termination reaction is carried out blowing, centrifugal, oven dry, pulverizing, extruder grain, packing.
Embodiment 3:
The preparation method of urea formaldehyde, its technical process is: add filtrate in reactor, be warming up to 60 ℃, add specified amount urea.Use 20%NaOH adjust pH to 8.6 after the stirring and dissolving.The formaldehyde that adds specified amount, described formaldehyde, urea ratio be 1: 1.2～1.5 this moment temperature rise to 77 ℃, with 20%NaOH adjust pH to 8.6, constant temperature kept 65 minutes.Open cycle cold water is cooled to 60 ℃ then, adds then between 20% the dilute sulphuric acid adjust pH 5.3, and constant temperature kept 12 minutes for 66 ℃; Between the dilute sulphuric acid adjust pH 4.7 of adding 20%, constant temperature kept 12 minutes for 66 ℃; Between the dilute sulphuric acid adjust pH 4.3 of adding 20%, constant temperature kept 12 minutes for 66 ℃.With 20%NaOH adjust pH to 8.6, cool the temperature to 30 ℃, termination reaction is carried out blowing, centrifugal, oven dry, pulverizing, extruder grain, packing.
Claims (1)
1. the preparation method of a urea formaldehyde, it is characterized in that: in reactor, add filtrate, be warming up to 60 ℃, add urea, use 20%NaOH adjust pH to 8.5～8.8 after the stirring and dissolving, add formaldehyde, described formaldehyde, urea ratio are 1: 1.2～1.5, this moment, temperature rose to 75～78 ℃, with 20%NaOH adjust pH to 8.5～8.8, constant temperature kept 60～70 minutes, and open cycle cold water is cooled to 60 ℃ then, add then between 20% the dilute sulphuric acid adjust pH 5.4～5.1, constant temperature kept 10～15 minutes for 65～68 ℃; Between the dilute sulphuric acid adjust pH 4.8～4.6 of adding 20%, constant temperature kept 10～15 minutes for 65～68 ℃; Add between 20% the dilute sulphuric acid adjust pH 4.4～4.1, constant temperature kept 10～15 minutes for 65～68 ℃, with 20%NaOH adjust pH to 8.0～8.5, cooled the temperature to 30 ℃, and termination reaction is carried out blowing, centrifugal, oven dry, pulverizing, extruder grain, packing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2007100718657A CN101260008B (en) | 2007-03-09 | 2007-03-09 | Method for preparing ureaformaldehyde |
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| CN2007100718657A CN101260008B (en) | 2007-03-09 | 2007-03-09 | Method for preparing ureaformaldehyde |
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| CN101260008A true CN101260008A (en) | 2008-09-10 |
| CN101260008B CN101260008B (en) | 2012-08-22 |
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| CN2007100718657A Active CN101260008B (en) | 2007-03-09 | 2007-03-09 | Method for preparing ureaformaldehyde |
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| CN102701862A (en) * | 2012-06-21 | 2012-10-03 | 深圳市芭田生态工程股份有限公司 | Compound fertilizer sustained release agent and preparation method thereof |
| CN103011982A (en) * | 2012-12-29 | 2013-04-03 | 山东金正大生态工程股份有限公司 | Industrial production method and device of urea-formaldehyde slow-release compound fertilizer |
| CN103304339A (en) * | 2013-06-29 | 2013-09-18 | 贵州省五谷惠生态农业科技有限公司 | Special fruit tree long-acting compound fertilizer production method of tree long-acting compound fertilizer special for fruit trees |
| CN103319237A (en) * | 2013-06-19 | 2013-09-25 | 山东天山丰耘生态肥业有限公司 | Method for producing three-in-one coated controlled release fertilizer |
| CN103524172A (en) * | 2013-09-30 | 2014-01-22 | 广西柳润物资有限公司 | Mixing and granulating method of urea formaldehyde, nitrogen, phosphate and potassium fertilizers |
| CN104261949A (en) * | 2014-10-23 | 2015-01-07 | 贵州省化工研究院 | Method for producing special long-acting organic-inorganic compound fertilizer for corn |
| CN104429860A (en) * | 2014-12-16 | 2015-03-25 | 五洲丰农业科技有限公司 | Seedling culturing substrate slow in nutrition release |
| CN104744082A (en) * | 2015-03-17 | 2015-07-01 | 安徽中农化工国际贸易有限公司 | Preparation method of urea formaldehyde powder |
| CN104892150A (en) * | 2015-05-27 | 2015-09-09 | 山东农业大学 | Instant slow-release nitrogen fertilizer and preparation method thereof |
| CN105315048A (en) * | 2014-05-30 | 2016-02-10 | 中化山东肥业有限公司 | Process for preparing urea formaldehyde slow-release fertilizer through diluted solution method |
| CN105503279A (en) * | 2015-12-24 | 2016-04-20 | 贵州省化工研究院 | Slow-release urea formaldehyde fertilizer and preparation method thereof |
| CN106565361A (en) * | 2015-10-08 | 2017-04-19 | 王兆博 | Process for producing general-purpose double-effect scientific fertilizer |
| CN108752075A (en) * | 2018-05-30 | 2018-11-06 | 广东隆戈尔生态技术有限公司 | The production method and production line of nitrogenous potassium dual-sustained-release composite fertilizer |
| CN114184000A (en) * | 2021-12-20 | 2022-03-15 | 武汉绿茵化工有限公司 | Urea formaldehyde continuous polymerization drying production device |
| CN114249621A (en) * | 2021-12-27 | 2022-03-29 | 清远市美村生物技术有限公司 | Special solid trace element fertilizer for golf lawn and preparation method thereof |
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| CN100368391C (en) * | 2005-06-16 | 2008-02-13 | 三通生物工程（潍坊）有限公司 | Crotonylidene diurea production method |
| CN100513359C (en) * | 2005-07-08 | 2009-07-15 | 上海化工研究院 | Method for preparing slow-release multielement compound-mixed fertilizer for forest trees |
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2007
- 2007-03-09 CN CN2007100718657A patent/CN101260008B/en active Active
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| CN102701862B (en) * | 2012-06-21 | 2014-02-19 | 深圳市芭田生态工程股份有限公司 | Compound fertilizer sustained release agent and preparation method thereof |
| CN102701862A (en) * | 2012-06-21 | 2012-10-03 | 深圳市芭田生态工程股份有限公司 | Compound fertilizer sustained release agent and preparation method thereof |
| CN103011982A (en) * | 2012-12-29 | 2013-04-03 | 山东金正大生态工程股份有限公司 | Industrial production method and device of urea-formaldehyde slow-release compound fertilizer |
| CN103011982B (en) * | 2012-12-29 | 2014-12-31 | 金正大生态工程集团股份有限公司 | Industrial production method and device of urea-formaldehyde slow-release compound fertilizer |
| CN103319237A (en) * | 2013-06-19 | 2013-09-25 | 山东天山丰耘生态肥业有限公司 | Method for producing three-in-one coated controlled release fertilizer |
| CN103304339A (en) * | 2013-06-29 | 2013-09-18 | 贵州省五谷惠生态农业科技有限公司 | Special fruit tree long-acting compound fertilizer production method of tree long-acting compound fertilizer special for fruit trees |
| CN103304339B (en) * | 2013-06-29 | 2015-01-07 | 贵州省五谷惠生态农业科技有限公司 | Special fruit tree long-acting compound fertilizer production method of tree long-acting compound fertilizer special for fruit trees |
| CN103524172B (en) * | 2013-09-30 | 2015-11-04 | 广西柳润物资有限公司 | The mixing granulation method of urea formaldehyde and nitrogen, phosphorus, potash fertilizer |
| CN103524172A (en) * | 2013-09-30 | 2014-01-22 | 广西柳润物资有限公司 | Mixing and granulating method of urea formaldehyde, nitrogen, phosphate and potassium fertilizers |
| CN105315048A (en) * | 2014-05-30 | 2016-02-10 | 中化山东肥业有限公司 | Process for preparing urea formaldehyde slow-release fertilizer through diluted solution method |
| CN104261949A (en) * | 2014-10-23 | 2015-01-07 | 贵州省化工研究院 | Method for producing special long-acting organic-inorganic compound fertilizer for corn |
| CN104429860A (en) * | 2014-12-16 | 2015-03-25 | 五洲丰农业科技有限公司 | Seedling culturing substrate slow in nutrition release |
| CN104744082A (en) * | 2015-03-17 | 2015-07-01 | 安徽中农化工国际贸易有限公司 | Preparation method of urea formaldehyde powder |
| CN104892150A (en) * | 2015-05-27 | 2015-09-09 | 山东农业大学 | Instant slow-release nitrogen fertilizer and preparation method thereof |
| CN106565361A (en) * | 2015-10-08 | 2017-04-19 | 王兆博 | Process for producing general-purpose double-effect scientific fertilizer |
| CN105503279A (en) * | 2015-12-24 | 2016-04-20 | 贵州省化工研究院 | Slow-release urea formaldehyde fertilizer and preparation method thereof |
| CN108752075A (en) * | 2018-05-30 | 2018-11-06 | 广东隆戈尔生态技术有限公司 | The production method and production line of nitrogenous potassium dual-sustained-release composite fertilizer |
| CN114184000A (en) * | 2021-12-20 | 2022-03-15 | 武汉绿茵化工有限公司 | Urea formaldehyde continuous polymerization drying production device |
| CN114184000B (en) * | 2021-12-20 | 2022-11-08 | 武汉绿茵化工有限公司 | Urea formaldehyde continuous polymerization drying production device |
| CN114249621A (en) * | 2021-12-27 | 2022-03-29 | 清远市美村生物技术有限公司 | Special solid trace element fertilizer for golf lawn and preparation method thereof |
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| CN101260008B (en) | 2012-08-22 |
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